Process of heating column-stills.



E. GUILLAUME.

PROCESS OF HEATING COLUMN STILLS.

APPLICAHON FILED MAY 24. 1910.

1,199,371. PatentedSept. 26,1916.

2 SHEETSJ-SEEET 1.

WHNESSES: h NVENTQR M wm 1. BY 2 I a ATTORNEY EIGUILLAUME.

PROCES S 0F HEATING COLUMN STILLS. APPLICATION FILED MAY 24.71910.v

1,199,371.- S Patented Sept. 26,1916.

2 SHEETS-SHEET 2.

' WITNESSES: LNVENTOR I ATTORNEY.

' tion and distillation,

tion alone, where the system embraces a puin elevation, of an embodimentwherein disfor distillation and rectification in a UNITED STATES PATENTOFFICE.

EMILE GUILLAUME,

OF PARIS, FRANCE.

PROCESS OF HEATING COLUMN-STILLS.

ing elements of another under regulated pressure; all as more iullyhereinafter set forth and as claimed.

The subject matter of the present invention is certain improvements madein the heating of a rectifying or secondary column still in apparatusfor distillation and rectification, whether such apparatus be adapteddirect and continuous manner, or whether continuous separaterectification is utilized. These improvements, which are a developmentof certain improvements disclosed in my prior Patent No. 887,793 ofMay'l9, 1908, are in part applicable in distillation organizations andmethods such as are disclosed in said patent and are also particularlyapplicable in other apparatus for continuous rectificaor continuousrectificarifying column for phlegms of low strength.

In the case of continuous separate rectification in the distillery, thatis where the distilling and rectification though effected in the sameplant are separate operations, in the present invention the vapors ofdistillation are caused to pass through a heating element which, for thepresent purposes, is also a condenser, arranged in heating relationshipto a rectifying column still. With this arrangement, the heating elementis, as stated, a condenser and takes the place of the condenser usuallyemployed with the primary still, thereby enabling the saving andutilization of much of the heat ordinarily wasted in such condenser. Atthe same time the arrangement gives a desirable type of heating of thesecondary or rectifying still.

It is to be noted that in the present invention where the wine, etc.,forming the raw material is to be preliminarily heated this instead ofbeing done by a heat interchanger abstracting heat from the still prod-Specification of Letters Patent. Patented Sept. 26, 1916. Applicationfiled May 24, 1810. Serial No. 563,105. v

ucts, must be done by a special heating arrangement, as by placing awort warmer at the head of the rectifying column, since the usualheat-interchanger at the head of the primary still is necessarily doneaway with.

In the case of direct and'continuous distilling and rectifyingsystemsembracing a primary or wine still, a purifying column for low degreephlegms, a continuously operating rectifying still and a column for theexhaustion of the wash, in the present invention the vapors coming fromthe primary pass through special connections to and from the heatingelements of the rectifying column before going to the low degreepurifying column, which must be sultably 1ocated in the system.

The distilling and rectifying operations may be conducted much as usual,as regards the special operative methods, and as if comletely separated,but the heat of the vapors rom the primary still is utilized in lieu ofbeing sent to waste. Rectified alcohol may be obtained of the samecharacter as that produced by separate operation of the two classes ofstills.

In the accompanying illustration I have shown more or lessdiagrammatically certain typical embodiments of apparatus elements ofthe many embodiments adapted for employment in the stated process.

In this showing, Figurel 1s a view, mainly .an'ordinary tubular type inthe base of rectifying column C. From the base of B, lead a trapped pipe2 and a pipe 3, respectively carrying condensate and vapor. The latterpipe is valved at a and has a valved by-pass 5 connecting it with thevapor line 1. By suitabl manipulation of valves t and 5, the amount andpressure of the vapors passing into B can be controlled. Pipe 2, in thisfigure, provides continuous removal of condensed liquid withoutdisturbance of these through vapor line 1 omitted but is desirable sinceotherwise the return liquid flow would necessarily beinto the top of theexhausting column proper. Elements 1010' designate as a wholeconnections for removing fusel oil and. collecting the same by means ofpipes t, t'- and .,coolers a, u in testing devices '0, o. Element 11 isa flask or separator for separating the vapors and liquid emerging fromB. Elements 12, 13 and 14 are heat-indicating devices, such asthermpmeters or thalpotassimeters, which allow regulation of theoperation. The vapor and liquid from.

B pass, in this embodiment of the invention, into the condenser orcooler 15, provided with testing'device 16, for the raw phlegins.Element 17 is a preheater for the Wine or other liquid to be distilledin the primary still A; and may be of any ordinary type; 18 is aheat-economizer or preheater for the raw phlegms fed to purifying columnD; 19 and 20 are steam regulators controlling, respectively, the heatingof the primary still A and of the exhausting column E; the steam flowingby regulator 19 in the path indicated by arrows s 8 and by 20 asindicated by arrows 8 -8 Element 21 is a phlegm vat for receiving thecondensed phlegms of the primary still.

In the operation ofthe described apparatus, the raw wine or otheralcoholic liquid passes through preheater 17 into A (as indicated byarrows a and b) where it is distilled in the ordinary manner, theenriched alcoholic vapors passing through 1 into B (arrow 0) where theyare in part condensed, following the direction of arrow (11. By the aidof valve 1 the pressure, and consequently the heat, may be controlled inthe heating element of rectifying column C. Valved by-pass 5 allows theshunting of any desired fractional amount of vapors from 1 into vapor pie 3 (arrow 6) without going through B so that the amount of heatdelivered to B can be thus controlled. Valve 4 and b v-pass 5 allow adelicate regulation, such as is necessary in a rectifying column, of theheat delivered to C. The heating power of the vapors coming from theprimarv still A is of course a function of their alcoholic richness, arich vapor being at'a lower temperature than a Such a portion of thevapors from the prima r v s1 ill A as is not necessary or desirable inheating the rectifying column C is simply to rectifying '(Z to testingd. from the purifying column D to the exhaustthrough 9 (arrow 0) ditionof poorer vapor. I

shunted or by-passed through 5 and. the condenser 15, (arrow f) therebyallowing regulation of heating without embarrassing the operation of theprimary still A.

It is in all cases desirable in running a rectifying column that anample amount of heat' be supplied but that this amount be controlled andregulable. -Too much heat produces obstructionv of the plates of thecolumn. I

.Ilhe liquid'phlegms from 15 may be delivered to the vat 21 and thencethrough 18 (arrows z' and j) to purifying column D which is providedwith the usual condensers and accessory parts,d d d 41*. Arrow 7c showsthe course of vapors from D to d arrows Z and Z show the course ofcondensate coming from d and (Z and arrow m shows the course ofcondensate from cooler Purified phlegms pass ing column E. The materialpasses through pipe 6 as shown by arrow a. To E is also suppliedwashfromrectifying column C and the alcoholic vapors pass into E through 7(arrow 30). Column C is also provided with the usual condensers andaccessory parts, these parts beingv marked 0 c 0 and 0*. Arrow 9 showsthe course of vapor going from C to 0 and arrows r and 7 show the courseof condensate returning from c and 0 Arrow 8 shows the course ofcondensate through cooler 0 and tester 0 i In the modification shown inFig. 2 distill-ration and rectification are continuous o goes to goingthe system of Fig. 1. Like elements of the two figures are designated bylike reference characters. In this modification, the phlegm cooler (15)is omitted and the described outlets from B deliver vapor and liquidinto purifying column D. The same by-pass and valves exist, by-pass 5establishing the shunt communication with the vapor from vapor line 1which can pass therethrough to D without having to pass from abovedownward through the tubular heating element. This by-pass may, as shownin Fig. 2, communicate with the heating element chamber in line withelement 1, or may communicate directly by a pipe connection with element1, as in Fig. 1.

It is necessaryto have a difference in level between B and the inlet 6for purified phlegms into the column E, and this may be taken advantageof, as shown, by the adconcentrating section E 11S concentrating sectionhas the advantage of raising the concentration of the alcoholic vaporsdelivered into the base of the rectifying column and of the boiling bodyof liquid therein, and, thereby, of allowing the use of richer vapors inthe heating element without necessitating an intermediate condenser, asin the system disclosed in the e knowledged Patent-887,793., Italsoallows;

the extraction of fusel oils outside the'rec tifying column, as atlO. I

boiling liquid in the base of. B, theg lower is the boiling point andconsequently, the

greater is its condensing power on the vapots in B. The tubesacannotbecomejhotterthan the boiling point of the liquid. g Onitheother hand,correlatively, withthijsfrichnessi increases the heatingpower; of the'phlegm; vapors on the body of boiling liquid. 1: Un-- der atmosphericpressure, the temperature of the vapors emitted from a boiling liquidof8 Gay-Lussac, for example, is 93.9 C. while the temperature of thevapors from liquids of 40, 80 and 90 Gay-Lussac will be, respectively,841, 79.92 and 79.12 C.

With the extraction of fusel oil per- 'formed (as by element 10) atthebaseof the interposed intermediate section E-, the zone of maximumconcentration of the fus'el oil is removed from the heater-condenserfBand the rectifier C.

As to the quantity of'steam or heat neces-' sary to exhaust the washin'column E, it

may be pointed out that the interposition of section E does not afiector increase this.

E has no influence upon the liquidwhich enters E from 6 and passesdownward so far as good exhaustion of such liquidin-E is concerned. Aneconomy is thus possible between this amount of steam and that which therectifying column requires while obtaining the very high concentrationof 965 to 97 Gay-Lussac in the upper plates of the latter. The economy"of steam 'should I in fact easily reach 100 kilos of steam perhectoliter of alcohol of 100 Gay-Lussa'c.

In Fig. 3 is shown a modified form of my 4 invention asregards thearrangement of the heater-condenser and its'c onnections and' re lationsto the rectifier, as well as the-connections ofthe latter tothe column Efor ex-. hausting wash.- The elements having the.

reference characters found in Figs. land 2 are the same in functionwhile additional elements have other reference characters.

In Fig. 3 the heater-condenser B has been somewhat modified in form tomake it a comparatively long; cylinder, affording. a comparativelylongpassage for the phlegm vapors. The liquid connection of 2 with theheater instead of being at a single point is afiorded through aplurality of. branched connections 2 2 and 2 tapping at dilfere entpoints. Pipe 2, as in Fig. 2, delivers (arrows g g and 9 to thepurifying column D (arrow g) at a pointjust above the inlet of pipe 3,and above a platejust above said inlet.

A difference over Fig.

ing column section E with the rectifier C at a higher point (arrow p).Asshown, this connection .isseveral plates higher than -B .and -isfnotimmediately above B, as in The richer the alcoholic content of theReflux 22, valved zit 2 6 allowsretrogrestioniof vaporsto be. attainedin E.- A coinplementary retrogre ssionwof liquid is efi'ect- .ed,.asbefore, by 8 and 9. (arrow 0), delivjering from apointat'the top oftheheatercondensertB'toxa 'low point in E,Land in the immediate vicinity ofthe .point where removal ofufusel oil and tail products isbeingefi'ected': by 10. By manipulation of cock 26,);the total amount ofi retrogressing liquid passing through22 and 8'9 can be controlled so asto correspond to that'going through .819 in Fig. 2.

:ltl'eait indicator, 'or thermometer or thalpotassimete'r '21", is forobserving the char acter ofthe operation in E ,while 23and 2 5,respectively, indicate thepressure prevailing in Band the low'er part ofG. Pipe 27, valved at 24, allows a direct e'xitf(arrow for phlegm vaporswhen it is "desired to use'such vapors to heat a columnor col umns' forfinalrectification, as=in the inven-l tion disclosed in my copendingapplication SenNo. 367,697, filed Aprilll, 1907. In event of. theabstraction of vapors-for this purpose, pipe 28 may be provided for thereturn i of condensate from the heater-condenser (arrow y) to the liquiddelivery pipe dot the presentheater condenser.

In the structure "of-'Fig. 3 of the present case, upper section E isnot, as in Fig. 2, continuous with the lower section E, but is aseparate element. For convenience of illustration E, which must be on alevel low enough to receive the purified phlegms coming from-'purifier D(here shown fragwmen'tally) is not shown. Pi es 29'and 30 are providedfor connecting F arrows c and e the upper or concentrating sectlon E.with the lower section E.

What I claim is:-

1. In the distillation of alcohol, the process which comprises formingcomparatively rich alcoholic vapors from comparatively weak alcohol ofcomparatively high boiling relationship to stronger alcohol of lower 7boiling point to distil and rectify the same p v I comparatively Weak"alcohol compara 2 is in the connecv tion of the vapor lead 7 from theexhausttively' high boiling. point, passing a controlled fraction ofsuch current 1nto heatimparting relationshlp to stronger alcohol point,passing a current of such vapors un- Ider controlled pressureintoheat-imparting Ill of lower boiling point to distil and rectify thesame, separating the uncondensed from the condensed vapors of suchfraction after so passing and uniting the uncondensed vapors with theresidue of the said current.

3. In the distillation of alcohol, the process which comprises formingcomparatively rich alcoholic vapors from comparatively Weak alcohol ofcomparatively high boiling point, leading a current of the vapors intoheat-imparting relationship to stronger alcohol of lower boiling pointto distil and rectify the same, separating the condensed liquid from theuncondensed vapors of such currentafter such heat-imparting relationshipand passing the condensed liquid and ethe uncondensed vapors into acolumn still to produce such stronger alcohol.

4. In the distillation of alcohol, the process which comprises formingcomparatively rich alcoholic vapors ,from comparatively weak alcohol,leading a current of such vapors under controlled pressure intoheatimparting relationship to stronger alcohol to distil and rectify thesame, separating the condensed liquid from the uncondensed vapors ofsuch current after so passing and passing the condensed liquid and theuncondensed vapors into a column still to produce such stronger alcohol.

5. In the distillation of alcohol, the process which comprises forming acurrent of alcoholic vapors, diverting a controlled fraction of saidcurrent intoheat-imparting relationship to stronger alcohol to distiland rectify the same, separating the uncondensed vapors from thecondensed liquid of such fraction after this diversion, reuniting theuncondensed vapors with the residue of the original current and passingthe current and the condensed liquid into a column still to produce suchstronger alcohol.

6. Inthe distillation of alcohol, the process which comprises distillingand rectifying a body of comparatively strong alcohol by a current ofweaker alcoholic vapors passed in heat-imparting relationship theremoved liquid and returning the concentrated vapors to mingle with thevapors above said body.

7. In the distillation of alcohol, the process which comprisesdistilling and rectifying a body of comparatively strong alcohol by acurrent of weaker alcoholic vapors passed in heat-imparting relationshipthereto but out of contact therewith, separating the condensed liquidfrom the uncondensed vapors of such current after so passing and passingthe same into a purifying still, removing the liquid from said purifyingstill, removing liquid from said body, producing concentrated alcoholvapors from the removed liquids, and mingling said vapors with thevapors from the rectifying of said stronger alcohol during therectification.

8. In the distillation of alcohol, the process which comprisesdistilling and rectifying a body of comparatively strong alcohol with acurrent of Weaker alcoholic vapors passed into heating relationshipthereto but out of contact therewith, transmitting the condensed anduncondensed vapors into a purifying column still, removing liquid fromthe purifying still and producing con-- centrated alcoholic vaporstherefrom in a column, passing said vapors through a concentratingcolumn at a higher level, and passing the vapors from the concentratingcolumn into admixture with the vapors from said body, liquid from saidbody being also supplied to the top of said concentrating column.

In testimony whereof, I have signed my name to this specification in thepresence of two subscribing witnesses.

EMILE GUILLAUME.

\Vitnesses:

JULEs FAYOLLET, DEAN B. MAsoN,

